CN1118995A

CN1118995A - Improved distillative separation process by steaming for mixtures of multiple substances

Info

Publication number: CN1118995A
Application number: CN94191401A
Authority: CN
Inventors: 威尔弗里德·拉斯; 约翰·F·菲斯; 凯瑟琳·帕兹; 汉斯·谢克; 约瑟夫·科兹玛; 罗尔夫·威德米耶尔
Original assignee: Henkel AG and Co KGaA
Current assignee: Henkel AG and Co KGaA
Priority date: 1993-03-06
Filing date: 1994-02-25
Publication date: 1996-03-20
Also published as: EP0687192A1; CZ215995A3; KR960700785A; CA2157660A1; JPH08507464A; PL310531A1; WO1994020187A1; DE4307115A1; AU6207194A

Abstract

The present invention relates to a process for intensifying and/or accelerating the distillation-based separation of multicomponent mixtures using a stream of steam to facilitate the removal of steam-volatile components of the starting material (''streaming''), characterized in that a starting material which is liquid under the treatment conditions is steamed in finely sprayed form. The process is preferably carried out with superheated steam under the working pressure which, more particularly, is at least partly used as a propellent gas for spraying the liquid phases to be purified. The material to be processed is best sprayed in multicomponent spray nozzles using this propellent gas. The process according to the invention may be used for a broad range of applications by adaptation of its parameters, more particularly the working temperature and pressure.

Description

By improving one's methods of decatize separated multicomponent mixture

The present invention relates to a kind of method of separated that adopts vapor stream to strengthen and/or accelerate to the multicomponent mixture in the organic source of small part, with the steam-volatile component that promotes to remove raw material.The invention particularly relates to and be used to belong to the generally purification step of the industrially scalable of " decatize " scope at large.But operation principle of the present invention has surpassed it in this application on the one hand.The present invention relates to the separated of extremely general raw material, particularly can be used as the separated of the raw material that is in a liquid state under the condition of work of distilling auxiliary agent at steam.

Be used to separate organic mixture, especially the steam distilled operation principle of corresponding utility or its mixture of purifying is the long-term chemical knowledge of setting up, referring to as L.Gatterm-ann " Die Praxis des organischen Chemikers ", the 33rd edition (1948), Walter De Gruyter﹠amp; Co.Verlag, 26-28 and 252 pages.Wherein, consequently it only can mention several characteristics application at this paper to be applied to various industrial circles for the described principle of laboratory practice in so different mode.

The purification of plant or zoogenous fat and oil comprises the multistep processing, and wherein the decatize of pre-raw material of purifying is normally carried out as one of final step.The purpose of the key technology of this specially treated step is the pre-raw material of purifying of deodorizing.The impurity of the useless especially stench that will be usually only exists with trace by steam distillation is removed from the mixture of useful material or useful material.But steam also can be used as the distillation auxiliary agent.For example promote SCFA from natural fat and oil, to remove.To this, in following document, be described, as " Ull-manns Encyklopadie der technischen chemie ", the 4th edition, 11 volumes (1976), 479-486 page or leaf; Kirk-Othmer " Encyclopedia of chemicalTechnology " the 3rd edition, the 9th volume (1980), in " Oilseeds Oilsand Fats ", II rolls up (1983) for 816-820 page or leaf and E.Bernardini " Vegetable Oils and Fats Processing ".Interstampa-Rome, VII chapter, 221-251 page or leaf (Deodorization of Fats and Oils).Purification process described in the document is with industrially scalable, presses steam distillation, and more definite operating under vacuum and high temperature by the decatize principle carried out.For example, decatize is to carry out under the temperature of 2-30 millibar and 150～290 ℃.Employed quantity of steam and processing time decide by selected special process.Batch process, semi-continuous process and continuity method are known.In all these the whole bag of tricks, steam is to be passed in fusion and the overheated fat or oil with finely divided form.In semicontinuous and continuity method, also can provide other auxiliary agent to increase steam and the surface between the oil phase of waiting to purify.

Nearest publication comprises D.Osteroth " Taschenbuch fur Lebensmit-tel chemiker und-technologen " the 2nd volume, Springer Verlag, Berlin, 1991, the 101-103 pages or leaves.This publication is particularly related to by decatize and adopts steam distillation or reextraction to remove the modern crafts that scent of and have the material of taste in a vacuum in fat and oil refining.The related in this case material that has taste and scent of mainly is to follow other volatile component such as free fatty, sterol, the aldehydes of tocopherol etc. and ketone.Relate to equipment, the decatize process can semi-continuously or continuously be carried out discontinuously promptly in batches.Continuous process more and more is used because of its PR is higher.Preferred processing pressure is about 2～5 millibars, and treatment temperature is 240-260 ℃, and this depends on the type of oil.Using the falling liquid film backflow device of nearest new development then can make the consumption of steam reduce to minimum, for example is 1～3% of oil mass.For fear of wastewater problem, must set up and comprise the vapor stream of removing organic principle.

But above-mentioned purification is said more precisely, and deodorizing is important for raw material not only.Chemical synthesis and the product that is obtained by the natural source chemical conversion also need this class purification step.The processing of aliphatic acid, aliphatic alcohol and its product, especially at cosmetics, the purification of the liquid ester that is suitable for handling in medicine and the field of food during this time mentions it being for giving an example fully.Below fully for listing indivedual representatives for example: Guerbet alcohol, oleate, soya-bean oil epoxides, nutmeg isopropyl propionate, glyceryl triacetate etc.

Industrialized other the typical aspect that adopts decatize to purify is to remove the oxirane in the product and/or the residue of expoxy propane base, and this product is to produce by the ethoxylation of the organic compound that contains at least one active hydrogen atom and/or propoxylation.Such compound is extremely important, for example as non-ionic surface active agent or as the intermediate product of producing anionic surfactant compound.They for example are used to, and detergent applications also is used for cosmetics and pharmaceutical adjuvant field on a large scale.In it was produced, the initial product that obtains contained oxirane and/or expoxy propane and the undesirable secondary response product such as the diox of trace.From oxyalkylated derivative, remove these residues and be reasonable need and key step in the production process.In this case, the product of initial acquisition is used to remove the steam distillation of not wishing to have impurity, more precisely decatize, it is the processing step that carries out industrially scalable, referring to for example EP-A1-028 3862, DE-A1-3447867, US-PS-4143072 and document cited herein.

Yet, in the improvement of the above-mentioned operation principle of mentioning, also can heat the useful material to be purified or the mixture of useful material, preferably in a vacuum, then they are carried out partial concentration by the steam distillation principle by evaporation and purification.For this reason, knownly use auxiliary, randomly overheated steam.In case of necessity, can be then that the water content that obtained is lower but do not have the process product of impurity to change into aqueous compositions, referring to for example DE-A1-3044488 and DE-A 3343802, the production method of the ether sulfuric ester that reduces diox content has been described wherein.

People also know the purification of the mixture of organic useful material and organic useful material, and especially its deodorizing and/or the impurity do not removed not can adopt uncondensable gas phase to carry out as the distillation auxiliary agent.In this case, preferably distilling auxiliary agent is gaseous nitrogen, and it can be used for promoting more volatile component to remove from mixture, consults for example J-AS-5414/81.According to the document, make poly-(alkylidene) diol, derivatives (for example as emulsifying agent, lubricating oil is used for plastics by under 90～100 ℃/30 torrs, gaseous nitrogen or steam being injected liquid to be purified, washing agent, the raw material of cosmetics etc.) purify and deodorizing.Recently also the someone is proposed in the deodorizing aspect of above-mentioned edible oil of mentioning and/or fat, uses uncondensable inert gas, and nitrogen especially replaces steam and as the reextraction auxiliary agent, consults for example EP-A2-015739.

US-PS-4443634 has described the method for purification of aliphatic alcohol polyglycol ether, wherein in material spray to that will be the to be purified chamber, can be removed by vapor form by this chamber impurity.The document has been described the respective mixtures conduct raw material to be purified that will contain the impurity (is base with the liquid charging stock) that will remove less than 2% (weight).It is said that material to be purified is sprayed in the inert atmosphere, selection pressure will be convenient to form the drop of size between 50～100 μ m.It is said about several seconds in these drop contact inert atmospheres, collect then.Mention nitrogen in the literary composition, helium and argon can be used as inert gas.The impurity that will remove through this spraying processing is oxirane, expoxy propane, diox, water and alcohol especially.In the continuous processing step, also liquid phase repeatedly can be sprayed in the inert atmosphere.

In its early stage German patent application DE-A 4237934, the applicant has described a kind of improving one's methods, to improve wetting agent, the purity of useful material and useful mixtures of materials in washing agent and/or cleaning product (raw material) field, especially smell and tinctorial quality, it is characterized in that the steam treatment with overheated is loaded with the raw material of impurity, in raw material, use bleaching agent to improve color.In a preferred embodiment,, particularly use the superheated steam that mixes with water with the raw material that is loaded with impurity acinous superheated steam, in case of necessity to small part be dry handling.This processing with superheated steam is preferably carried out in spraying area and/or fluid bed.Thereby the early stage German patent application DE-A 4237934 of disclosed this piece of writing specially lists in this article as part disclosed by the invention.

This earlier application is based on surprising observation, significantly sense of smell improvement in the raw material of especially described type, as disclosed in its early stage document and German patent application with applicant's name, can principle with superheat steam drying obtains by applying to impure raw material.For example, by also can reach very effective deodorizing and final corresponding centrifugation with superheat steam drying.

Information with the principle of superheat steam drying can be found in following patent literature and the early stage German patent application with applicant's name: DE-A 4030688, DE-A 4204035, DE-A 4204090, DE-A 4206050, DE-A 4206521, DE-A 4206495, DE-A4208773, DE-A 4209432 and DE-A 4234376.According to the present invention, as hereinafter defined, by distilling enhancing and/or promoting the method for the separation of multicomponent mixture to be based on the discovery and the working rules of DE-A 4030688 and the early stage German patent application of mentioning.Therefore, the document and cited earlier application are all specially listed in this article with as part disclosed by the invention, so that understand in conjunction with hereinafter described further discovery and working rules.

Before going through the inventive method, mention the commercial Application of complete different field below earlier below, to help to understand steam distilled principle.As everyone knows, by using the steam distillation principle can simplify inconvenient separation based on distillation.For example in EP-B-0092876 and other corresponding application, described in the product at non-ionic surfactant component and from alkylpolyglycosides (APG) class, removed unreacted aliphatic alcohol.According to the document, the distillation that contains the raw product of APG is carried out under vacuum in thin layer evaporator.Pass through the vapor stream of this evaporimeter by having raw material (raw material being diffused on the inner surface of the thin layer evaporator) contact that has increased the surface, can promote removing of free-fat family alcohol to be distilled.

Thereby, first embodiment of the present invention relates to the separated that adopts vapor stream to strengthen and/or accelerate to the organic multicomponent mixture of small part, with the steam volatile component (hereinafter being referred to as " decatize ") that promotes to remove raw material, the raw material that it is characterized in that being in a liquid state under treatment conditions is with thin spray form decatize.In the method for the invention, decatize is handled and is carried out with superheated steam under operating pressure.In the embodiment of a particular importance, liquid phase to be purified is sprayed with auxiliary propellant gas, in order to reach this purpose, particularly advantageously be to adopt multi-component nozzle.In this embodiment of the present invention, overheated steam is used as propellant gas at least in part.

But in improved method, the raw material liq of essentially no at least water under condition of work can be sprayed to does not have in the auxiliary flow of superheated steam of propellant gas.This embodiment is characterised in that propellant gas useless, simplified superheated steam and the separation of the required specified quantitative ratio between the raw material of waiting to purify, and infringement is not easy to any advantage that quality is transmitted, this can give the credit to the surface that increases greatly, and the quality transmission is the continuous phase that passes on from one to another peripherad superheated steam under operating pressure from the organic liquor of thin spray.

In another embodiment, the present invention relates to the application of this method in various technical fields.A key area relevant with the present invention is to purify, and especially fat and/or oily deodorizing is so that they for example can be used as food, are used for cosmetic field and/or are used as pharmaceutical adjuvant.The Another application field is to produce flavor enhancement product and flavor enhancement concentrate.

Another important use is to be used to improve wetting agent, the useful material of the plant in washing agent and/or cleaning formulation field and/or synthetic source and the purity of useful mixtures of materials, especially for handling fabric, for example cloth-washing detergent, cosmetics and/or pharmaceutical adjuvant.

More particularly, the present invention relates to adopt the mixture of described method, especially remove impurity with purify oxyalkylated useful material and oxyalkylated useful material, as the residue of unreacted EO.PO or its secondary product as 1, the 4-diox.

In addition, the inventive method relates to the hereinafter extremely general application of described operation principle, is used as the distillation auxiliary agent in the separation of the mixture that do not volatilize to small part.

The critical aspects of the inventive method is following change: in the deodorizing of traditional fat and oil, for example pass through batch process, the liquid for the treatment of deodorizing is imported as continuous phase at first, and the steam that will be used for decatize simultaneously is with finely divided form input and by continuous liquid phase to be purified, for example the star with a plurality of exit passageways by being used for steam or the injected system of annular or other shape.The inventive method has changed this principle fully.And the raw material that will under treatment conditions, be in a liquid state be input to the contact of finely divided shape steam mutually in, steam forms continuous phase usually.

The result of this change has increased the liquid surface of the pending liquid phase of unit volume greatly, and it is the key from the mass transfer in liquid phase to the vapour phase.For example, the crucial ratio liquid surface of quality transmission can be according to 10 ²～10 ⁵The factor, on average be about 10 ³The factor and increase.

According to purpose of the present invention, the form with this liquid phase existence for the treatment of decatize that increases the surface in fact finally can strengthen and/or quicken the separation of the steam supporting of multicomponent mixture.And for traditional decatize, as pressing the decatize of one-step method to fat and oil, the required processing time for example is 6-10 hour, even in the general continuity method of high speed development, the required processing time still is several hours, by adopting step of the present invention after several approximately seconds, just can obtain final purification result.The advantage that this method has is fully aware of.It can not only finish employed technical process very apace, can also control the temperature that raw material to be purified contacts within the specific limits safely by the present invention.The liquid for the treatment of deodorizing can be by original known method spraying.The vast scope of the relevant technology aspect one pack system and/or multi-component nozzle and method and technological parameter all can be used for this purpose.Need not make the raw material for the treatment of deodorizing keep the long time of staying, when especially adopting second principle of the present invention hereinafter described at atomize.In case of necessity, gas to be purified can be repeated several times to the transformation of thin atomize and the interaction of continuous vapor phase.In single spray step, can use used steam and/or live steam.The spraying circulation that repeats can be carried out in individual unit or a plurality of continuous unit of separating.Even in the method that use repeats to spray, the time of pending raw material contact high temperature (if any) is no more than a few minutes.Especially the employing of employed condition of work, particularly operating pressure and temperature and optimal selection also have nothing to do in separating step.

Technology of the present invention also provides batch operation or continued operation.The case description of the particular of the inventive method will discuss in more detail in accompanying drawing 1-3 hereinafter.

Obviously, can adopt critical process principle mentioned above, it is used suitable to depend on pending Material Characteristics with best special process pressure.Therefore, the decatize of spraying area can normal pressure or decompression or even under superpressure, carry out, this depends on the volatility of pending raw material and the impurity that will remove.Aspect decatize, above-mentioned open and specific data of the prior art are to be applicable to this respect basically.

Select specific operating pressure to determine the boiling temperature of the water under the condition of work.According to the present invention, under specific operating pressure, carry out decatize with overheated steam.Thereby, preferably under normal pressure, keep the temperature of vapor phase more than 100 ℃.In this respect, employed vapor (steam) temperature is a particular importance.The specified temp that is used for superheated steam and selects is subjected to many parameter influences, says more precisely by many parameter decisions.The parameter of the key of this respect comprises the volatility of steam for example and is transformed into the amount of the component of vapour phase by pending multicomponent mixture.But generally speaking, another factor that should consider is the temperature sensitivity of pending raw material.As following described in detail, the inlet temperature that also should consider to enter spraying area.Certainly, as what discuss among the DE-A-4030688 that begins to mention, principle below aspect the superheated steam spray-drying, having adopted: under the boiling temperature that is being lower than water under the operating pressure, be sprayed in the overheated steam if will treat the raw material of decatize, overheated steam condensation raw material at first naturally in cooler, with the transfer of heat of condensation in the raw material of thin spray, so that under condition of work, make single drop be heated to the boiling temperature of water.Only reach the boiling temperature of water according to the object of the invention in single drop, then decatize is just carried out effectively.Temperature Distribution in such single spray droplet is desirable fully, and optionally sets up under concrete condition.But generally be that the raw material that will treat decatize is sprayed in the vapor phase of minimum temperature, this minimum temperature is equivalent to the boiling temperature of water at least basically under operating pressure.

Under the particular job pressure that purification step is selected, the temperature of superheated steam preferably is higher than 10-30 ℃ at least of the boiling temperature of water, more preferably is higher than at least 50 ℃.Short of basic obstruction, for example owing to treat the caused result of temperature sensitivity of decatize raw material, so employed vapor (steam) temperature can be higher significantly.Therefore, the temperature of suitable steam can be higher than at least 100 ℃ of the boiling temperatures of water under the operating pressure of purification step, preferably is higher than 150-200 ℃ at least.

Consider the parameter that adopts by the expert in this respect, the temperature sensitivity of pending multicomponent mixture for example, vapor phase and the mass ratio for the treatment of decatize fluid multi-component mixture etc. can adopt quite absolute vapor (steam) temperature.These operating temperatures of steam (now with condition of work under the boiling temperature of specific water separate) for example can be up to about 500 ℃, be preferably 100～400 ℃, only at the raw material of handling high temp. sensitive, this raw material for example contains and to be lower than under 100 ℃ the temperature (vapor (steam) temperature of use is lower than 100 ℃) component of mixture that is easy to wreck.In this case, steam treatment must be carried out in enough vacuum certainly.

Relate to the prior art of this class, the abundant reference of operating pressure and vapor phase temperature best of breed is provided through the purification step of decatize.According to the relevant document of above enumerating, natural fat and the oily deodorizing known by decatize are to carry out under the condition of decompression greatly, for example at 1～20 millibar, are higher than 100 ℃ high material temperature and adopt simultaneously, for example 150～270 ℃.Method of the present invention also comprises the combination of this class limit of temperature and pressure certainly; Although generally will select inlet temperature to be higher than fluid temperature, the temperature of employed superheated steam is equivalent to treat the fluid temperature of decatize basically, in case of necessity even can be lower than this temperature.Obviously by general professional knowledge, particular of the present invention, its is set up certainly can import other evaporation energy by employed superheated steam, and to remove by vapor phase acceleration and/or enhancing raw material aspect optimum is provided.

Therefore, in the method for the invention, the free-pouring material to be purified that particularly exists with liquid phase under operating temperature is sprayed in the steam flow of preferred superheated steam, and liquid phase is separated from this vapor phase basically.Can find included useful especially design procedure hereinafter in the discussion of Fig. 1 of accompanying drawing-3.The mentioned above special circumstances relevant with particularly preferred embodiment of the present invention are discussed in advance.

In embodiment of the present invention of mentioning, liquid phase to be purified is sprayed by means of propellant gas.The various structures of corresponding aerosolizing part, more particularly nozzle is known in relevant prior art, consult for example H.Brauer " Grundlagen derEinphasen-und Mehr-phasenstromungen " in GRUNDLAGEN DERCHEMISCHEN TECHNIK, Verfahrenstechnik der Chemischem undverwandter Industrien, Verlag Sauerlander, Aarau und Fran-kfurt am Main (1971), the 308-323 page or leaf; A.H.Lefebvre " Atomizati-on and Sprays " Hemisphere Publishing Corp.New York (1989), the 10-20 page or leaf; Chemical Engineering, the 2nd volume, Unit Operation (nineteen sixty-eight the 2nd edition), Perergamon Press, Oxford/New York, 602-617 page or leaf; With people such as R.H.Perry in " Chemical Engineering Handbook " (1975 the 5th edition) MacGraw-Hill Book company, New York " Phase Disp-ersion/Liquid-in-Gas Dispersions " 18-61 is to the 18-62 page or leaf.

Particularly preferred embodiment of the present invention is to use multi-component nozzle and propellant gas.In the most important embodiment of the present invention, superheated steam is to be used as propellant gas at least in part.

In the above-mentioned difficult point of the present invention that this paper mentions, most important embodiment is to use superheated steam as unique propellant gas, to spray liquid multicomponent mixture and convert it into the liquid phase of final dispersion.Wonderful discovery is used as the propellant gas place at superheated steam, strengthened component to be separated from the transmission (this chances are along with spray process strengthened the cause of mixing) of liquid phase, to such an extent as to just can in the special process circulation, reach the purification result in second part to the superheated steam phase.Mode of operation of the inventive method and advantage are understandable.Consider the formation ad hoc approach of the spray droplet of describing in the listed document, the stratiform that wherein generally comprises liquid phase is disperseed, and to form layer as thin as a wafer, it is understandable that enhancing degree of the present invention just purifies the result.In addition, the technology personnel of general professional knowledge in the scope of the inventive method by selecting suitable multi-component nozzle can strengthen this effect.

In one embodiment, by method of the present invention, in the spraying of liquid phase to be purified, in fact employed all steam can both be used as propellant.But in an important embodiment, by part steam, especially superheated steam can set up and keep the predetermined direction of vapor phase stream again in addition in the spray chamber.For example, the reative cell of arranged vertical is counter-current operation in such a way, be about to liquid along with the superheated steam as propellant gas is sprayed downwards, and the steam of part flow of superheated steam makes progress towards the raw material adverse current of spraying simultaneously.

According to the present invention, the specific characteristic of the inventive method and make according to the disclosed close relation with superheat steam drying of other earlier application of DE-A-4030688 and the above-mentioned applicant who enumerates might be by purify anhydrous basically raw material and handle water-containing material with superheated steam at spraying area of decatize, so as the purifying by decatize can with combine to the small part drying.

Begin to be mentioned as this paper, the important improvement of the inventive method is characterised in that liquid, and main at least the waiting Organic Ingredients of purifying carefully is sprayed in the steam flow of superheated steam, and do not use the propellant gas of superheated steam base.Superheated steam has separately especially reduced the employed superheated steam amount of organic liquid of purifying of waiting of every base unit as the working media in the spray process (can use one-component nozzle in the known manner in this embodiment).Drop size by adjusting the organic liquid of will spraying is in the known manner also set up superfine spraying liquid, can quicken from the quality transmission of continuous phase of the peripherad superheated steam of liquid phase of spraying, even in this embodiment, reach in several approximately seconds, can obtain useful purification result, or also can reach approximately under the few cases a few minutes.More particularly, can use in the described particular in several steps bringing into operation, in step in succession, eliminate influencing each other of running parameter simultaneously in case of necessity.If adopt this class multistep method, then organic liquid phase is sprayed to continuous superheated steam these two operation principles in mutually as propellant gas spraying and without propellant gas where necessary even can combine each other with overheated steam.

The selected parameter relevant with prior art with the operating parameter of the particular job step of using is consistent among the present invention.Therefore, the operating pressure of selection can be about 1～50 millibar, more particularly, if to be purified be for example fat and/or oil or natural source of low volatilization raw material, then operating pressure is about 3-30 millibar scope.Equally also be applicable to the elaboration products and/or the synthesis material of comparison low volatility.But in an important embodiment of the present invention, the purification of spraying area is at normal pressure or only be to carry out under moderately reducing pressure.In the specific embodiment preferred of the present invention, increase the density that quality is transmitted by using superheated steam as propellant gas, even when operating pressure is not lowered to necessary so far quite low value, usually can separate effectively.Can have the importance of simplification and saving equipment and running cost by the decatize purification.

The required specified quantitative of superheated steam is decided by selection and its degree that stands to heat and the selected special process of parameter, the especially raw material that will consider.Usually, for the embodiment that adopts superheated steam as propellant gas, employed quantity of steam is to wait to purify about 1～30% (weight) of material, is preferably about 5～20% (weight).Do not use superheated steam to do in the embodiment of propellant gas using one-component nozzle, then quantity of steam is particularly advantageous by treating that the decatize raw material is counted 2～10% (weight).For the embodiment of not using propellant gas, specially suitable raw material is anhydrous at least basically.The water content of organic useful material will be lower than 10% (weight), is preferably lower than 5% (weight), and it is preferred especially being lower than 1～3% (weight).

Average droplet size acceptable scope in technology of spraying material for example is 20-500 μ m, especially 50-200 μ m.Processing time in the particular job step is approximately several seconds as mentioned above, can increase the processing time by the multistep operation, though in this case with general steaming method, even with the form of its high speed development relatively, the processing time remains extremely short.

Fig. 1-3 with reference to accompanying drawing has described the principle of the invention, wherein relates to the processing of anhydrous basically raw material.

Fig. 1 and 2 schematically illustrates the deodorizing in batches of material, and this material is liquid state and sprayable under operating temperature.By selecting specific device suitably, deodorization process can be carried out under normal pressure and under the decompression in batches.

Fig. 1 has illustrated the deodorizing in batches in jar 1, and tank skin is adiabatic and/or is furnished with heating system 2.At the top of jar demister 3 is arranged, for example with filler (packing) form of corresponding vapor permeable, it arranges to have one or more nozzles 4 down.Under illustrated situation, the multi-component nozzle of nozzle for operating as propellant gas with superheated steam.With part steam by manage 5 and superheater 6 be transported in the multi-component nozzle 4.In case of necessity, also part steam can be transported in the components distributor 7 of jar 1 bottom.Liquid 8 that will be to be purified by pump 9 passes through pipe 10, randomly extracts out from the bottom of jar 1 by heat exchanger 11, and is transported in the nozzle 4.The superheated steam that is loaded with impurity that is passed in the vapour phase is extracted out by pump 13 by pipe 12.Overheated steam can be controlled cooling in heat exchanger 14 and 15, so that the condensation portion of the material extracted out is removed by 16,17 and 18.After the raw material 8 of fully purifying by decatize according to the present invention, can remove batch of material and also the new a collection of raw material of waiting to purify is input in the device by managing 19.

Deodorization process in batches in the post that Fig. 2 illustrates is corresponding with its key element illustrated in fig. 1.But, for example between the lower nozzle 4 of jar 1 and liquid phase 8, be furnished with in addition in the filling unit 20 of the modern splitter known type that is used for distilling and absorbing as the sepa-ration aid of auxiliary phase.Corresponding metal and/or plastics filling unit are the working cells of standard, particularly in splitter by distillation, absorb and resolve the unit that is used to separate, referring to being entitled as of Gebruder Sulzer AG " Trennkolonnen fur Destillationund Absorption " (be used to distill and adsorb splitter) " separate edition Produ-ktbereich Chemtech Trennkolonnen; Winterthur, Switzerland (22.13.16.20-V.91-100).

Separation of material can promote by one or more unit 20 shown in Figure 2 even be easy to the separation of the liquid and gas in the post of mixture foamy in processing.In the device shown in this and Fig. 1, in fact the amount of the liquid 8 of jar 1 bottom can be selected on demand.

Multistep decatize of the present invention is shown in Fig. 3, and this is based on continued operation.

Optional heatable post 21 is divided into three parts by the unit 22 and 23 that is enough to vapor permeable.The separative element 22 of vapor permeable and 23 can by known method for example by suitable sieve plate or even bubble cap tray etc. form.Separative element 22 and 23 effect are to stop fluid product to be assembled in its surface on the one hand, and by pump 25 (top of post) tying-in pipe 24 or will be passed in the lower reative cell through managing 27 liquid phases that are input to first nozzle 28 by pump 26, so that liquid phase can be removed in the bottom of splitter specific part, and pass on again on demand.

To heat in heat exchanger 29 through managing 24 crude products of carrying by pump 25, and be entered into the top of post 21.To be loaded with and treat that deimpurity working steam (it is to flow out from the top of post 21 by conduit 30) at first exchanges once more fully with the liquid of newly importing at the upper top of post.For this reason, in Fig. 3, is furnished with bubble cap tray 31.Reliable separation the between the gas phase in the impure steam that this resolution element is particularly useful for guaranteeing to rise and liquid phase.On sieve plate 22, nozzle 28 places are extracted and directly be transported to liquid by pump 26 out through managing 32, here liquid phase by through conduit 33 and 34 inputs as the overheated live steam of propellant gas and thin spray.Through the hydraulic shock separative element 35 of spraying, this separative element 35 is shown among Fig. 3 once more as bubble cap tray, and implements to separate for the first time between gas phase and liquid phase.The gas phase that rises is passed through sieve plate 22, and extracts out from splitter through conduit 30 and heat exchanger 37 by pump 36.

Liquid phase is left at it and is collected than the separative element 35 of low side and by sieve plate 23.The continuous liquid phase that to collect by pump 39 is pumped into the next spraying area with nozzle 40 by conduit 38 then.In this spraying area, liquid phase is handled by the live steams of conduit 33 and 34 inputs once more according to the present invention's use.The liquid phase of spraying in this processing section is impacted packing layer 42.Reference above Fig. 2 is observed, and corresponding filler 20 also can be used for this processing section.

Flow through downwards filler 42 and be collected in the bottom of splitter of the liquid of having been purified in two sections now here, can be handled it with overheated live steam once more, and steam is through conduit 33 and 43 and be transported on the distributor 44.

By pump 46 liquid of purifying is cooled off by the crude product of discharging and use input in 45 of column bottom in heat exchanger 29, and remove by 47.

For Fig. 1 and 2 two figure and Fig. 3, operating pressure can be selected and regulate in the intended manner in the inside of splitter on demand.Pump 13 and 36 is particularly suitable for pressure is adjusted to about normal pressure or vacuum.High-volatile reason owing to the individual product component.If desired can be in excessive rolling work, pump (25,26,39 and 46 among 9 among Fig. 1 and 2 and Fig. 3) is the operation element that is specially adapted to carry liquid product flow.

Mentioned as beginning, the invention provides to the processing of anhydrous material basically with to the processing of water-containing materials.The general requirement of carrying out the inventive method is under condition of work, is especially adopting under the condition of superheated steam as propellant gas, and this method should be the pending multicomponent mixture of as far as possible carefully spraying on technology.These embodiments of the present invention relate to the corresponding water-containing material of use and by the method for hereinafter describing in detail of the present invention it are handled.

People will recognize at once can be divided into the present invention several specific embodiments.This is because Material Characteristics on the one hand, especially relates to the feature of its water content and the physical characteristic of anhydrous useful material or anhydrous useful mixtures of materials under condition of work and standard conditions.Be the versatility of the possible specific embodiments of deriving from the present invention on the other hand: the present invention not only tries hard to realize the separation on the general deodorizing meaning, and the drying of useful material or useful mixtures of materials also can comprise within the scope of the invention.Therefore, employed specific device largely is to be decided by the correlation of specific material and the purpose that will realize with the mensuration of carrying out under individual cases.By the general professional knowledge of the present invention and background technology provided by the invention, can be easy to see the wide wide range of application of process of the present invention.The example of individual characteristics is described below, and integrality is had no requirement.

In first specific embodiments, raw material (it wants dry under treatment conditions, preferably be not easy to the impurity of steam volatilization) moisture under the condition of work can be handled by the present invention.But, basically by context of the present invention, even can be considered as separated with from moisture useful material or moisture useful mixtures of materials, removing to anhydrate, the result even can represent one embodiment of the invention by adopting superheated steam to quicken drying as the propellant gas that is used for carefully spraying raw material (preferably by suitable multi-component nozzle) in this case., particular aspects of the present invention makes it to carry out simple drying.Such as this concrete condition, seldom run in practice.The useful material that runs in the industrially scalable operation or the type of useful mixtures of materials often contain the impurity of trace at least, and these impurity are in the decatize of the inventive method and discharge by vapour phase in the drying steps simultaneously.This is specially adapted to the above-mentioned useful material and the purification of useful mixtures of materials, these materials are taken from wetting agent, washing agent and/or cleaning formulation field and relevant with the useful material discussed among applicant's the early stage German patent application DE-A-4237934, and this application is as the open part and listing in of the present invention.In the embodiment of this earlier application, adopt nitrogen pending slurry also to be used the superheated steam counter-current drying by two component nozzle spray as propellant gas.But according to the present invention, superheated steam is directly as propellant gas.Can improve and quicken the purification and the drying of used mixture basically like this.

More particularly, above cited early stage patent application is the solid-state material through purifying and the product of the mixtures of materials through purifying after also relating to drying.Now, the present invention expands the moisture and sprayable preparation of useful material of this class or useful mixtures of materials to.Obtainable result and last appreciable parameter are the purposes that above begins the early stage German patent application DE-A-4234376 of cited applicant in this class material of processing.Therefore, it is open and once more as part disclosed by the invention to list this earlier application in.This earlier application has been described the microcellular structure of how developing and being fixed on in the material of superheat steam drying, and the mixture of how being discussed by unknown so far method preparation based on this respect from the useful material of product.

In the embodiment of just having mentioned, the inventive method comprises by decatize the purification of used useful material or useful mixtures of materials and the drying of used aqueous compositions is combined, and has considered the key element of the early stage German patent application DE-A 4234376 of applicant simultaneously.

Therefore, the invention particularly relates to a kind of method, the method is characterized in that to use and flow freely the solid-state useful material of sprayable aqueous compositions shape or the mixture of useful material, it is to be suitable under decatize and overheated drying condition, even under the condition of contacted vapours, form solid, this solid has the internal structure of perforate, and its plasticity and surface viscosity are restricted to such degree so that the perforate of its particle and/or internal structure be prevent greatly adhering to each other.Relevant with the mixture that is processed with material or useful material, particularly importantly adopt water miscible and/or fine grain water-insoluble inorganic and/or organic additive, it is preferably solid-state and be not clamminess in its drying regime.

, in second embodiment, the present invention also comprises the useful material of the under household condition free-pouring aqueous compositions form of processing or the mixture of useful material.Under this condition, to the separation of undesirable steam volatile component can be advantageously with superheated steam wholly or in part drying combine.The product (under household condition being in a liquid state) that an example of this type material is the moisture alkoxylation of compound, it is the compound that comprises at least a reaction hydroxyl, for example, the aqueous compositions of corresponding non-ionic surfactant component.The maximum application of this class alkoxylation comprise substantially remove fully exist in the elaboration products as the formed residue of secondary alkoxylation product, for example, oxirane (EO) and/or expoxy propane (PO) and undesirable cyclic ethers, for example diox.The present invention just provides these undesirable trace impurities of effective separation and dry simultaneously initial water-containing materials to predetermined extent in single method.

Consider general professional knowledge, just can recognize in all cases at once that the processing method that will select and work apparatus should be suitable in advance by the definite condition of product property.All embodiments of the present invention should have thin spray property, say more appropriately, the spraying area that adopts superheated steam to be full of with the steam that forms the present invention's requirement as propellant gas.Under condition of work, keep the useful material of its flowability or the mixture of useful material to be sprayed once more in the first spraying section back, thereby and be transported in the multistage technology.Be converted to solids fraction, particularly the useful material of the solids fraction by synchronous drying or the mixture of useful material are not easy to be transported in second process section of process of the present invention.In this case, if carry out second active section, so at first the material of drying should be converted into the liquid preparation that can spray again.

In a preferred embodiment, the inventive method comprises that superheated steam to the small part that is loaded with the discharge component of raw material does not have those components of raw material after the feed separation of purifying.Like this can with useful material from be loaded with steam mutually separate and reclaim and/or can prevent waste water handling problem.But, also the water that contains of purifying can be recycled when needing.

The vapor phase that is loaded with impurity can form by the known any way of professional basically.General professional knowledge can be used for this purpose.Proved that second active section that membrane technology is used for the inventive method is effective especially.The representative of the general professional knowledge of this respect such as Ju.I.Dytnerskij " Membran-prozesse zur Trennung flussiger Gemis-che " (membrane processing method that is used for liquid mixture) " book " VEB DeutscherVerlag fur Grund-stoffindustrie, Leipzig, 1977 and M.Cheryan " ULTRAFILTRATION HANDBOOK ", Technomic Publishing CO., Inc., Lancaster, Basel, 1986.

According to the type and the characteristic of selected film, to select and adopt specific membrane separation process, the particular technology that is adopted is determined by specific mixture to be separated.The water that is loaded with impurity can be in single-stage, or even forms in multistage.The selection of suitable film can be by filtering by ultrafiltration and millimicro and carrying out in the microfiltration the hyperfiltration.Here specific technical step is also determined by the related parameter that has of mixture to be separated.

Figure 4 and 5 illustrate usually under normal conditions, the relevant possibility that contains the corresponding separation of water condensation phase, and this contains that water condensation communicated will be from the absorption of raw material separated portions and after the vapour phase condensation and assemble as liquid phase.

In Fig. 4, the formation of steam treatment of the present invention with exhaust steam that is loaded with impurity or waste water is combined.The steam treatment step is to carry out with in two sections of arranged in series, and the step of employing is as follows:

The material for the treatment of decatize by the top that heat exchanger 48 and conduit 49 are transported to jar, is carefully sprayed it by one or more nozzles here.Fresh steam is heated in heat exchanger 52 after the required operating temperature by conduit 53 is input in jars 50 the distribution units 54, and set up continuous superheated steam phase than lower part.To be near small part be input in the nozzle 51 by conduit 55 as the superheated steam of propellant gas another kind of possibility.

In the bottom of jar 50, the liquid of steam treatment is extracted out by pump 56 and is transported to the top of second aerosol can 59 by conduit 58 through conduit 57, is carefully sprayed by nozzle 60 here.With overheated live steam by conduit 61 be arranged in jar 59 distribution units 62 and be input to this spraying area than lower part.In addition, the superheated steam as propellant gas can be input in the spraying system 60 more whole or in part by conduit 63.The liquid of steam treatment is extracted out and can be removed by 66 from the bottom of second spraying area 59 by pump 64 through conduit 62.

The superheated steam that is loaded with the steam volatile component by managing 67 and shift out from the top of second jar 59 from the top of first jar 50 with by managing 68, and is transported in the condenser 69 and makes it condensation.The liquid of assembling is transported in the pans 70 by conduit 84.The water of the organic component that is loaded with discharge that will collect in pans 70 is extracted out from the bottom of pans 70 by

pump

72 and 73 through conduit 71, and be transported in the membrane separator unit 75 by managing 74, penetrant shifts out by semipermeable membrane 76 and by managing 77, and is transported in for example common waste water processing station.Can not shift out by managing 78 by the retentate of film, can with its by pump 73 through managing 74 and part circulation.Will take from the component of loop discharges by 79.Handle and the further utilization of these components of discharging from raw material is determined by its potential value through deodorizing according to the present invention.If they are useful materials, they can be further processed or can utilize again.But, also can be it be disappeared and ruins by for example burning.

At last, Fig. 4 shows the uncooled gas phase of assembling is how to handle in condenser 69.Under the effect of compressor, uncooled gas phase is input in the tower 82 that is loaded with solid absorbent by managing 81, and is fixed in this absorbent, the progressively desorb of the component that has absorbed is to be undertaken by the device of known method by second absorption tower.The component that absorbs for example can be transported in the storage tank 70 by managing 83, aforesaid then with handling by managing 84 condensates of discharging from condenser 69.

Fig. 5 has illustrated the membrane separation process that changes, and the employing superheated steam is used for the condensate from the liquefaction of above-mentioned rectifying section (not shown).Discharge the condensate of the superheated steam of component and be transported in the storage tank 70 being loaded with raw material, and through managing 71, by

pump

72 and 73 and be input in the first film segregation section 75 through managing 74 by managing 84.Penetrant is removed by semipermeable membrane 76 and by managing 77.Retentate leaves the first film segregation section by managing 78, and can be with it through managing the 74 part circulations and/or remove and further handle and/or disappear and ruin by managing 79 by pump 73.

The penetrant of the first film segregation section removed is transported in the storage tank 85 by managing 77, and through managing 86, by

pump

87 and 88 and manage 89 and be transported in the second film segregation section 90.Penetrant is removed by semipermeable membrane 91 and by managing 92, for example as the waste water of fully purifying.Retentate leaves this second film segregation section by managing 93, and can partly be circulated by pump 88 through managing 89.Simultaneously, just as described, can make retentate by managing 94 circulations and turning back in the storage tank 70 of the first film separating step.

In described two sections condensation method of purifications, it is useful especially being provided at the semipermeable membrane that increases segregation section aspect its separative efficiency in continuous segregation section.For example, first section microfiltration can be combined with the ultrafiltration or the millimicro filtration of next section.But second segregation section also can be based on hyperfiltration.The combination of ultrafiltration and millimicro filtration or ultrafiltration and hyperfiltration also is possible certainly.At last, it also is possible using more than mutually combining of two segregation sections.

Operation principle of the present invention is with a wide range of applications.Integrality is had no requirement, and following application proposes as an example: decatize more particularly is used for for example food, fat and/or oily deodorizing in cosmetics and/or the pharmaceutical adjuvant field; The purity of improving the useful material of plant and/or synthetic source and useful mixtures of materials is especially at wetting agent, the material in washing agent and/or cleaning product (for example they are used for the fabric treating field), cosmetics and/or the pharmaceutical adjuvant field; The above-mentioned impurity of mentioning type is more particularly removed in the purification of oxyalkylated useful material and the useful mixtures of materials of this class.

But the present invention that puts it briefly especially also is suitable for as the distillation supplementary means in separating to small part low volatility mixture.By adopting particular job condition, especially temperature and pressure, can use the separation principle of simplifying through steam distillation effectively.The free alkyl alcohol of excessive separation is the representative instance of the potential application of the present invention in the above-mentioned reactant mixture that runs into from APG produces.But, also can be quite simple in the next important use of the situation of exception, from raw material, effectively remove the residue of the water that other method is difficult to remove.Thereby the mixture of useful material of this class of efficient drying or useful material.Here obtaining by adopting its parameter, especially temperature and pressure by method of the present invention usually is difficult to carry out also expensive in traditional separation method and result that obtain.

Can be advantageously used in the possible embodiment of wide range with the auxiliary distillation of the steam method of the present invention that is basic separating mixture.The removal (wherein usually comprising suitable technological difficulties) of the difficult impurity of a small amount of and minute quantity, can be by the steam distillation separating mixture effectively and technically reach (a large amount of or even the raw material mainly measured should from bottoms, separate) simply.An one example is to reclaim spices, and this spices is to discharge in overheated vapor phase, then they is separated and recovery.

Embodiment 1

In reaction vessel, in 180～200 ℃, use catalyst and carry out the esterification of aliphatic acid and glycerine, (Myritol 318 with the formation olein ^R, the product of Henkel KGaA).The water that reaction is assembled at first under normal pressure, is removed then in a vacuum.Esterification finished in about 15 hours.Then in refining vessel that ester depickling, washing is also dry in a vacuum with 10% sodium hydroxide solution.After bleaching and filter as bleaching agent, in deodorization step, remove the aliphatic acid of residual volume with diatomite.

During to end, olein is passed through two component nozzle spray to adopting in the deodorant holder of superheated steam as the arranged vertical of propellant gas.Collect in ester and the pumped back nozzle at container bottom.Simultaneously, superheated steam is injected in the deodorant holder by the direction of injection system against liquid.Steam is discharged with the smell effusion material that is mingled with wherein by a vacuum system, and vacuum system is made of steam-jet ejector and water ring pump.The size of container and nozzle and operating parameter are shown in as in the following table 1.

Table 1 size 1, deodorant holder

Wide (mm) 300

High (mm) 12002, two component conical hollow nozzle diameters (mm), 1 operating parameter

Liquid:

Through-flow (kg/h) 10

Temperature (℃) 160

Steam (injection nozzle):

Through-flow (kg/h) 4

Pressure (crust) 4

Temperature (℃) 170

Vacuum:

Press (millibar) 4 in the container

Cooling water temperature (℃) 10

After two step deodorizing, the content of free fatty is reduced to 0.08% (weight) from 1.02% (weight).After the three step deodorizing, the content of free fatty is reduced to less than 0.01% (weight).In following table 2, to estimate the stink of olein with respect to the form of the numerical value of free fatty residual quantity (by weight percentage).

Table 2 deodorizing C ₈Aliphatic acid C ₁₀Aliphatic acid C ₁₂The aliphatic acid free-fat

The summation of % (weight) % (weight) % (weight) acid is 0.66 0.36＜0.01 1.02 (initial value) 2 steps 0.02 0.06 of deodorizing＜0.01 0.083 step≤0.01＜0.01-＜0.01 not

Embodiment 2

Step as described in example 1 above.With spermaceti octadecanol (Lanette O ^, HenkelkGaA) by two component nozzle spray deodorizing.

The spermaceti octadecanol is high saturated fatty alcohol, mainly is the mixture of cetanol and octadecanol.It is a kind of base substance of favourable skin, and the consistency coefficient that has the stable emulsifying characteristic for emulsification is in particular for the hair oil and the drug ointment of creme and acidifying.Short chain free alkyl alcohol (C by the production technology existence ₁₀-C ₁₄) owing to its objectionable odor reduces product quality.These fatty alcohols of 95% (weight) are removed in two step deodorization process.

Listed process conditions below:

The spermaceti octadecanol:

Through-flow 10kg/h

150 ℃ of steam of temperature:

Through-flow 4kg/h

Pressure 4 crust

150 ℃ of temperature

Pressure in the deodorant holder is decided to be 20 millibars.The performance data of thereafter in the form of sheets, tasteless spermaceti octadecanol is as follows: chain length C _10-120%

C ₁₄ 0.5％

C ₁₆ 49％

C ₁₈ 50％

C ₂₀The density 0.82g/cm that 50 ℃ of acid numbers of 54 ℃ of freezing points of 0.5% rising fusing point, 0.02 saponification number, 0.1 iodine number, 0.1 hydroxyl value is 21860 ℃ ³

Embodiment 3

Method is as described in embodiment 1 and 2.In this case, remove residual fat alcohol (the long-chain C that the poly-glycosides (APG) of synthesis of alkyl back is kept _12-18).

APG is by directly synthetic (one-step method) preparation, wherein will be in fatty alcohol indissoluble glucose directly with fatty alcohol reaction, and formation alkylpolyglycosides.Reactant mixture is made up of 30% (weight) APG and 70% (weight) fatty alcohol.Most of excess fat alcohol are removed under 10 millibars/160 ℃ in falling film evaporator.Residual fatty alcohol amount is 8% (weight).Requirement in the by specification is reduced to residual fatty alcohol content less than 1% (weight) in three step deodorizing unit.During to end, APG raw material to be purified is sprayed as the two component nozzles (diameter 1mm) of propellant gas by adopting superheated steam (160 ℃).Operating parameter is as follows: alkylpolyglycosides: 180 ℃ of steam of through-flow 10kg/h temperature: 160 ℃ of through-flow 3kg/h pressure 4 crust temperature

The viscosity APG slurry of assembling is removed from deodorant holder by the pulsation outflow.It is diluted with water to active principle content is 60% (weight) and bleaching.Because the short time stops in second step that fatty alcohol is removed under about 160 ℃ of high temperature, has only micro-browning.So, using H ₂O ₂During belaching aqueous APG slurry as long as the less work amount.Comprise in the moisture form of 50% (weight) active principle at it, the APG product flows freely at about 40 ℃.

Embodiment 4

Method is as described in the embodiment 1-3.Deodorizing soya-bean oil.Deodorizing is to remove undesirable effusion smell of a large amount of formation and produce the material of taste by oxidation and hydrolysis compound or enzyme reaction.Described material mainly is aliphatic, saturated and unsaturated C ₆-C ₁₀The aldehyde of series, aliphatic ketone (methylheptyl, methyl nonyl, methyl undecyl ketone etc.) also comprises low-molecular-weight aliphatic acid.In addition, blanching step provides the oil that the soil flavor is arranged.Hydrogenation has produced typical hydrogenation aroma and flavor.The soya-bean oil of hydrogenation comprises 37 kinds of volatile compounds at the most, mainly is senior aldehyde, ketone, lactone and alcohol.With soya-bean oil (T=240 ℃) by spraying as two component nozzles of propellant gas with superheated steam.The steam that is superheated to 170 ℃ (p=1 crust) is imported by syringe.Container pressure is 5 millibars.Circulate after 4 times, final free fatty acid content is 0.04% (weight).Sensory test is positive.

Embodiment 5

Method is as described in the embodiment 4.The deodorizing olive oil.The temperature of oil is 220 ℃.After 4 circulations, aspect aroma and flavor, reached desired quality.

Embodiment 6-11

Method is as described in embodiment 4 and 5.The employed oil of deodorizing, the container internal pressure (millibar) and the temperature of the oil by two component nozzles (superheated vapor is as propellant gas) sprayings are shown in the following table 3.

Obtained the sense of smell acceptable result after 4 circulations of material to be purified.

Table 3 embodiment oil type container internal pressure (millibar) oil temperature (℃) 6 rape seed oils, 6 240 7 peanut oil, 5 220 8 sunflower oils, 5 220 9 coconut oil, 4 18010 palm oils, 6 23011 palm-kernel oils 6 230

Embodiment 12

Method is as described in the embodiment 1.The caprylic/capric triglyceride that deodorizing is prepared as follows:

Glycerine under normal pressure, in 120-200 ℃, there is the following and C of existence of catalyst _8-10Fatty acid response and form three esters.Under the vacuum that improves, continue esterification then.About 14 hours of total reaction time.After in vacuum (10 millibars), removing excess fats acid under 210 ℃, under the identical operations condition, carry out decatize with nitrogen.The cooling product, bleaching is also filtered.(pressure in the deodorant holder is 5 millibars for two component nozzles, diameter 0.5mm, and superheated steam is as propellant gas) carries out deodorizing by spraying in overheated steam then, and condition is as follows: caprylic/capric triglyceride:

Through-flow 8kg/h

180 ℃ of superheated steams of temperature:

Through-flow 7kg/h

180 ℃ of temperature

Pressure 1 crust

Circulate after 5 times, product processed is scentless.

Embodiment 13 and 14

Method is as described in the embodiment 12.The raw material for the treatment of deodorizing is BS (embodiment 13) and isobutyl stearate (embodiment 14), respectively by C _16-18Fatty acid mixt and n-butanol/isobutanol preparation.

The initial temperature of ester to be purified and the pressure in the deodorant holder (millibar) are listed in the table below in 4.

In the temperature deodorant holder of table 4 embodiment ester ester

(℃) pressure (millibar) 13 BSs 210 10 14 isobutyl stearates 220 4

Elaboration products after 5 circulations are scentless.

Embodiment 15-21

As embodiment 4-14, by fatty alcohol and the fatty alcohol ethoxylate of two component nozzles (superheated steam is as propellant gas) to list in the superheated steam spraying deodorizing following table 5 against input in addition.In following table 5, treat the raw material of deodorizing, the operating pressure in its temperature and the deodorant holder (millibar) is shown in the following table 5.

Purified product after 5 circulations is gratifying.

In the deodorant holder of table 5 embodiment fatty alcohol/ethoxylized fatty alcohol raw material

Temperature (℃) pressure (millibar) 15 C ₁₆Fatty alcohol 150 10 16 C ₁₂Fatty alcohol 100 10 17 C ₁₄Fatty alcohol 120 10 18 C ₁₈Fatty alcohol 170 10 19 C ₂₀Guerbet alcohol 2EO 120 10 20 C _18-20Fatty alcohol 3EO 100 10 21 C _16-18Fatty alcohol 29EO 130 10

Claims

1, a kind of method that strengthens and/or accelerate to the separated of the organic multicomponent mixture of small part, it is by removing the component of the steam-volatile of raw material with promotion by decatize with superheated steam under operating pressure, it is characterized in that: the raw material that will be in a liquid state under condition of work is with thin Sprayable decatize, with the propellant gas assistant spray of superheated steam form.

2, the method as requiring in the claim 1 is characterized in that liquid phase to be purified is sprayed by multi-component nozzle.

3, the method as requiring in claim 1 and 2 is characterized in that under the operating pressure of purification step, and the boiling temperature that the temperature of employed steam surpasses water is at least 50 ℃, preferably at least 100 ℃, and more preferably at least 150～200 ℃.

4, the method as requiring among the claim 1-3 is characterized in that liquid to be purified is injected in the overheated vapor stream, and this liquid and vapor phase is separated from each other basically.

5, the method as requiring among the claim 1-4 is characterized in that the liquid for the treatment of steam treatment is being sprayed under the boiling temperature corresponding to water under the condition of work at least basically.

6, the method as requiring among the claim 1-5, it is characterized in that spraying area normal pressure or decompression or even in the excessive rolling operation, this depends on the volatility for the treatment of material and the impurity that will remove.

7, the method as requiring among the claim 1-6, the temperature that it is characterized in that liquid phase to be purified and employed steam is coadapted, and substantially the same at least temperature is preferred, and it is particularly preferred using the superheated steam than higher temperature.

8, the method as requiring among the claim 1-7 is characterized in that vapor (steam) temperature is paramount and reaches about 500 ℃, is preferably about in the 100-400 ℃ of scope.

9, the method as requiring among the claim 1-8 is characterized in that anhydrous basically material is carried out steam treatment.

10, the method as requiring among the claim 1-8 is characterized in that water-containing materials is handled with superheated steam at spraying area, and is in case of necessity, simultaneously that it is dry at least in part.

11, the method as requiring in claim 1-8 and 10, it is characterized in that handling being loaded with the liquid of useful material of impurity and/or aqueous solution, emulsion and/or the suspension of solid under the room temperature, this processing is a steam treatment and to dry two kinds of small part.

12, the method as requiring among the claim 1-8,10 and 11, it is characterized in that, will be under operating temperature the aqueous compositions of mixture of useful material solid or the useful material of this class carry out by the separation of steam treatment and the processing that combines with superheat steam drying.

13, the method as requiring in the claim 12, it is characterized in that the useful material of solid of its use aqueous compositions form or the mixture of useful material, the said preparation form is suitable for forming the solid with perforate inner structure under condition of work, wherein make plasticity and surface viscosity be restricted to the perforate that makes particle and/or its internal structure, in addition with condition that superheated steam contacts under also prevent basically adhering to each other.

14, the method as requiring among the claim 1-13, it is characterized in that using water-soluble and/or the water-insoluble inorganic and/or organic auxiliary material of fine grained, be preferably solid and be not clamminess, handle the mixture of useful material or useful material in its drying regime.

15, the method as requiring among the claim 1-14 is characterized in that raw material is carried out the multistep steam treatment, and the multistep of especially thin spray form is handled, and at least one step superheated vapor is used as propellant gas.

16, the improvement of the method that requires among the claim 1-14 is characterized in that the anhydrous material that will be liquid at least basically under condition of work is injected in the flow of superheated steam of not using propellant gas.

17,, it is characterized in that water content＜10% (weight) of raw material to be purified, preferably＜5% (weight), more preferably＜3% (weight) as the method for requirement in the claim 16.

18, the method as requiring among the claim 1-17 is characterized in that being loaded with the component of the Xiang Buhan of steam from raw material, preferably adopts membrane separation process after the vapor phase condensation.

19, the purposes of the method that requires among the claim 1-18 is used for steam treatment, is particularly useful for as food the fat of cosmetics and/or pharmaceutical adjuvant and/or oily deodorizing and be used to reclaim spices and concentrated spices.

20, the purposes of the method that requires among the claim 1-18, the mixture of be used to purify oxyalkylated useful material and oxyalkylated useful material is especially removed impurity, as the unreacted residual thing of EO, PO or its secondary product as 1, the 4-diox.

21, the purposes of the method that requires among the claim 1-18 is being used as the distillation supplementary means to the separation of small part low volatility mixture.

22, as the purposes of the method that requires among the claim 1-18, be used for improving from wetting agent, washing agent and/or cleaning products field, in particular for fabric treating field such as cloth-washing detergent, the useful material of plant in cosmetics and/or the pharmaceutical adjuvant and/or synthetic source and the purity of useful mixtures of materials.